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Seminar 2014 RTG "Functionalization of Semiconductors" Seminar 2014 San Sebastián, Spain, 31.07.2014 – 01.08.2014 Research Summaries supported by: Graduiertenkolleg 1782 „Functionalization of Semiconductors“ Workshop & Seminar San Sebastian, Spain, july 28th – august 1st Seminar program (august 1st): Topic area A: Nanoscale layer structures for the functionalization of Silicon 9.00 – 9.30: K. Jandieri "Band alignment at (GaB)(AsP) / GaP interface: Theoretical suggestions from different experiments" 9.30 – 9.50: P. Springer, S. W. Koch, and M. Kira "New Approach to Calculate Excitonic Wave Functions in Indirect Semiconductors" 9.50 – 10.10: R. Woscholski, M. Stein, M. Drexler, A. Rahimi Iman and M. Koch "Optical properties and carrier dynamics of III/V semiconductors" 10.10 – 10.30: N. Knaub, A. Beyer, P. Ludewig and K. Volz "Quantitative STEM HAADF analysis of dilute Bi containing GaAs" Topic area C: Control of functionalization 10.30 – 10.50: K. Werner, A. Beyer, K. Volz and W. Stolz "Atomic Processes during the MOCVD of Gallium on Si (001)" 10.50 – 11.10: J. O. Oelerich, A. Stegmüller, K. Werner, A. Beyer, R. Tonner, W. Stolz, K. Volz and S. D. Baranovskii "Computer Simulation of Growth Kinetics of Compound Semiconductors" 11.10 – 11.40: BREAK 11.40 – 12.00: M. Reutzel, G. Mette, M. Dürr, U. Koert and U. Höfer "Breaking the O-C-bond: adsorption of diethyl ether on Si(001)" 12.00 – 12.20: S. Laref and R. Tonner "DFT Calculations of TETRAHYDROFURAN on Si(001)-4x2" 12.20 – 12.40: A. Pick and G. Witte "Site-selective Perylene-Deposition onto Microcontact-Printed Organothiols on Au-surfaces" Topic area B: Nanoparticles 12.40 – 13.00: J. Eußner and S.Dehnen "Functional binary and ternary Organotin Chalcogenides" 13.00 – 13.20: N. Rosemann and S. Chatterjee "Time-resolved photoluminescence-studies on AuSn-X clusters" 13.30 – 13.40: A. M. Abdelmonem, B. Pelaz and W. J. Parak "ZnO Nanoparticles: Synthesis and surface Modification for Biological Applications" 13.40 – 14.00: U. Kaiser, N. Sabir, M. Schneider, D. Jimenez de Aberasturi, W. J. Parak and W. Heimbrodt "Energy transfer characteristics of Mn doped CdS/ZnS quantum dots" 3 Poster program (july 30th, 16.00 – 19.00): Topic area A: Nanoscale layer structures for the functionalization of Silicon E. Sterzer, A. Beyer, K. Werner, R. Straubinger, W. Stolz. C. v. Hänisch, J. Sundermeyer and K. Volz "Nitrogen incorporation in GaAs using alternative precursors containing As-N and Ga-N bonds" T. Wegele, A. Beyer, M. Zimprich, K. Jandieri, W. Stolz and K. Volz "Investigations Focused on the Local Composition Determination of Dilute Nitride Quaternary Material Systems Grown on Si-substrates" A. Ott, A. Beyer, A. Ruiz Perez, B. Kunert, W. Stolz and K. Volz "Investigation of antimonide-based materials grown on exactly oriented (001) silicon substrate" S. Gies, M. Zimprich, T. Wegele, C. Kruska , A. Beyer, W. Stolz, K. Volz and W. Heimbrodt "Optical Spectroscopy of Novel III-V-Semiconductor-Heterostructures" J. Kuhnert, P. Ludewig, K. Volz and S. Chatterjee "Photo-modulated reflection and temperature-dependent photoluminescence studies of Ga(AsBi) bulk and quantum well structures" C. Berger, U. Huttner, M. Mootz, M. Kira, S. W. Koch, J.-S. Tempel, M. Aßmann, M. Bayer, A. M. Mintairov, and J. L. Merz "Microscopic Theory of Semiconductor Lasers" L. Kraft and H. Jänsch "An NMR-Approach to semiconductor burried interfaces" Topic area B: Nanoparticles N. Sabir, P. del Pino and W. J. Parak "Mn doped CdS, CdS/ZnS Nanoparticles Synthesis and characterization" B. Pelaz and W. J. Parak "Surface modification of nanoparticles" P. del Pino and W. J. Parak "Smart Particles for Bio-Apps" J. P. Eußner and S. Dehnen "Functional Binary and Ternary Organotin Chalcogenide Clusters" Topic area C: Control of functionalization A. Ostapenko and G. Witte "Preparation and characterization of phosphonic acid based self-assembled monolayers on Zn0 substrates" M. Lipponer, N. Armbrust, M. Dürr and U. Höfer "Reaction dynamics of exemplary organic molecules on Si(001) - a molecular beam study" A. Stegmüller and R. Tonner "MOVPE" Growth Phenomena of III/V Semiconductor studied by DFT P. Rosenow and R. Tonner "DFT-Study on the Adsorption of MOVPE-Precursors on III/V Semiconductors on Silicon and on Properties of III/V-Semiconductor Quantum Well Materials" 4 Topic area A: Nanoscale layer structures for the functionalization of Silicon New MOVPE Precursor Molecules for Highly Efficient Casting of Nitrogen into III-V Semiconductor Materials Wolf Schorn, Katrin Schlechter, Eduard Sterzer, Kerstin Volz, Wolfgang Stolz, Jörg Sundermeyer Faculty of Chemistry, Faculty of Physics and Materials Science Center, Philipps Universität Marburg, Hans-Meerwein Str. 4 and 6 1. Introduction Within our GRK 1782 research project A1 we are aiming to develop new volatile MOVPE precursor molecules that combine group 13 (B, Al, Ga, In) alkyl and hydride functionalities with an anionic low molecular weight N,N-chelate ligand motif. The goal is to lower the high activation barrier, the high deposition temperature and the large excess of ammonia or other nitrogen sources typically needed during casting of substantial amounts of N atoms via MOVPE into the GaAs and InP growth process, and into meta-stable III-V semiconductor materials, in particular. 2. Results 2.1 Design, Synthesis and XRD Structure Determination of MOVPE Precurors The low energy of N-N bond cleavage in hydrazine has prompted us to use 1,1- dimethylhydrazine (DMH), an established nitrogen source in MOVPE, as building block for volatile and even liquid boranes, alanes, gallanes and indanes. In order to stabilize these covalent molecules, we established the class of N,N’-bis-dimethylamino-acetamidine (BDMA) substituents. Our ligand synthesis follows a condensation of an active iminoester of acetic acid with two equivalents of DMH [1] (Scheme 1): Me Me 2 Me2NNH2, NEt3 HCl Me2N NMe2 HN OEt N N H H-BDMA Scheme 1: Synthesis of H-BDMA The reaction of Me3M (M = Al, Ga, In) with H-BDMA leads to elimination of methane and formation of low-melting, subliming and pentane soluble inorganic ring compounds Me2M(BDMA), which were characterized via single-crystal XRD analyses (Fig. 1). 7 Me2Al(BDMA) Me2Ga(BDMA) Me2In(BDMA) m.p. 41 °C m.p. 47 °C m.p. 47 °C Figure 1: XRD structure analyses of Me2M(BDMA) precursor molecules The synthesis of corresponding group 13 hydrides is a challenging goal outlined in our GRK proposal. The absence of any metal-carbon bond in the precursor minimizes the danger of undesired carbon incorporation during the MOVPE process. This problem becomes immanent in the presence of the lighter elements boron and aluminum. The binary hydrides are hazardous gases (B2H6), non-volatile polymers [AlH3]x or thermally (> -30°C) highly unstable compounds Ga2H6 or [InH3]x. We found, that our BDMA ligand stabilizes molecular ternary hydride compounds of these elements. Most of them are non hazardous liquids easy to condense. Our synthesis process chain for hydrido boranes, alanes and gallanes is displayed in Scheme 2 [1,2]: Unregistered PLT 4 LiH + GaCl3 LiAlH4 - LiCl NR3HCl -LiCl, -H2 LiGaH4 GaCl , Et O -LiCl, -H 3 2 2 R3N-AlH3 Et2O-GaH3 NMe2 NMe2 NMe2 NMe2 Me Me H Me Me N N N N H H H Al Al Ga - H , -OEt N - H , -NR N H N N H 2 2 N 2 3 N N N H Me Me Me Me Me Me Me Me H-BDMA H2Al(BDMA) H2Ga(BDMA) THF-BH3 NMe2 - H2, -THF NMe2 Me N Me N H H-BDMA, 120 °C H B B N H - H2 N H N N H3B Me Me Me Me H2B(BDMA) Scheme 2: Synthesis of group 13 hydrides stabilized by BDMA Single-crystal XRD structure analyses were performed at low temperature in order to evaluate the monomer or dimer nature of these molecular hydrides (Fig. 2): 8 H2B(BDMA)(BH3) H2Al(BDMA) H2Ga(BDMA) Figure 2: XRD structure analyses of H2M(BDMA) precursor molecules 2.2 MOVPE Studies The liquid H2Ga(BDMA) precursor was synthesized on a 20 gram scale, purified, condensed into a bubbler and used in MOVPE studies [4]. Nitrogen incorporation was determined by XRD measurements (X-Ray Diffraction). We achieved a GaNAs/GaAs growth of up to 0.8% N in combination with conventional Ga and As precursors (TEGa, TBAs) as shown in Fig. 3. The origin of the observed growth rate increase is interpreted as an efficient MOVPE process incorporating not only N but also Ga from the new precursor. Growth conditions without TEGa during GaNAs growth confirmed this interpretation. Room temperature photoluminescence (PL) measurements (Fig. 4) of not annealed sample show the expected band gap shift per % N. No TEGa 0,8 0,9 N Incorporation Growth rate 0,7 0,8 0,7 0,6 0,6 0,5 0,5 0,4 0,4 0,3 0,3 0,2 Growth rate (in nm/s) N Incorporation %) (in 0,2 0,1 0,1 0,0 0,0 0 200 400 600 800 1000 Flow Ga(BDMA)H2 (in ml/min) Figure 3: With increasing H2Ga(BDMA) flow, N incorporation and the growth rate increase. The encircled data points represent the sample without TEGa. 1 500 ml/min + TEGa 1 1000 ml/min +TEGa 500 ml/min without TEGa 0,1 0,1 0,01 0,01 Corrected (a.u.) Intensity 1E-3 1E-3 1,0 1,1 1,2 1,3 1,4 1,5 Energy [eV] Figure 4: Room temperature PL measurements on not annealed samples (same as shown in Fig. 3). 9 3. Conclusions We have managed to establish a new class of group 13 alkyls and hydrides suitable for synchroneous nitrogen and group 13 metal gas phase epitaxy at relatively low deposition temperatures.
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